CN104831268A - Preparation method of composite alloy coating on tantalum-tungsten alloy - Google Patents
Preparation method of composite alloy coating on tantalum-tungsten alloy Download PDFInfo
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- CN104831268A CN104831268A CN201510159203.XA CN201510159203A CN104831268A CN 104831268 A CN104831268 A CN 104831268A CN 201510159203 A CN201510159203 A CN 201510159203A CN 104831268 A CN104831268 A CN 104831268A
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Abstract
The invention relates to a preparation method of a composite alloy coating on a tantalum-tungsten alloy. The preparation method comprises the following steps of 1, MoSi2 coating slurry preparation, 2, MoSi2 coating high-temperature sintering, 3, Hf-Ta alloy coating slurry preparation, and 4, Hf-Ta alloy composite coating sintering. According to the preparation method, the product surface is spray-coated with the prepared MoSi2 coating as a transition layer, and the surface of the transition layer is spray-coated with an Hf-Ta alloy coating. The preparation method solves the problem of Hf-Ta alloy coating and base material bonding and tantalum-tungsten alloy high-temperature oxidation. The prepared composite alloy coating is uniform and compact, has no defects such as holes and cracks and has good oxidation resistance.
Description
Technical field
The present invention relates to high-temperature oxidation resistant coating field, particularly relate to the composite alloy coat preparation method on a kind of tantalum-tungsten alloy.
Background technology
Multiple rail control/attitude control engine material and high-temperature oxidation resistant coating has progressively been developed abroad from the 1950's, base material mainly concentrates on refractory metal (W, Mo, Ta, Nb, Re etc.) research, coating mainly concentrates on alloy coat, oxide coating, silicide coating, aluminide coating and noble coatings, as the niobium hafnium alloy/silicochromium titanium coating of the U.S., Muscovite niobium tungstenalloy/molybdenum silicide coating, the platinum rhodium thrust chamber in Europe, the rhenium iridium thrust chamber of the U.S. all has model application report.
Although current domestic rhenium/iridium material development achieves major progress, the application of distance through engineering approaches still has a segment distance.The over-all properties that tantalum-tungsten alloy is excellent, makes it be expected to reach development demand within a short period of time.Carry out the large quantity research of tantalum-tungsten alloy oxidation resistant coating abroad: as Royal company and Sylvania company etc.; Matrix material sci-tech research production community of Russia also have developed Mo-Pd coating and MoSi
2+ HaSi
2protective coating.
The domestic research being engaged in tantalum-tungsten alloy oxidation resistant coating is less, Shanghai silicate carried out the correlative study work of coating, the silicide families of coatings performance of preparation is 2.5 hours 1800 DEG C of life-spans, 1800 DEG C-room temperature thermal shock about 80 times; The silicide coating that the coloured Yuan Xiao state treasure in northwest waits people to prepare, 1800 DEG C of life-spans can reach 6 hours; The people such as Li Zhengxian adopt electrochemical plating to prepare Ir coating on tantalum-tungsten alloy surface, and only there are 15min in 1700 DEG C of life-spans.
The above-mentioned domestic tantalum-tungsten alloy oxidation resistant coating research carried out, general performance not high (1800 DEG C of life-spans were lower than 6 hours), some preparation method is also very complicated, can not meet the heatproof requirement that new work engine is higher.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, provide the preparation method of the composite alloy coat on a kind of tantalum-tungsten alloy, this preparation method's technique is simple, and be easy to realize, the coating uniform prepared is fine and close, has good antioxidant property.
Above-mentioned purpose of the present invention is mainly achieved by following technical solution:
A composite alloy coat preparation method on tantalum-tungsten alloy, comprises the steps:
Step (one), be the MoSi of 65% ~ 75% by mass percentage content
2powder and mass percentage content are the HfB of 25% ~ 35%
2powder mixes, and puts into ball mill and is dry mixed more than 4h, adds binding agent afterwards and MoSi made by thinner
2coating slip, slip more than wet mixing 1h in ball mill;
Step (two), the MoSi that step () is obtained
2coating slip is sprayed into product surface to be sprayed, the product to be sprayed sprayed is put into vacuum high temperature furnace and sinters, and sintering temperature is 1850 DEG C ~ 1900 DEG C, insulation 10min ~ 20min, during sintering, in vacuum high temperature furnace, vacuum gauge pressure is less than 0.1Pa, heats up and terminates furnace cooling, make MoSi
2coating;
Step (three), by mass percentage content be 75% ~ 85% Hf powder and mass percentage content be 15% ~ 25% the mixing of Ta powder, then add Y
2o
3powder and the mixing of Si powder, wherein Y
2o
3the quality of powder is 0.5% ~ 1% of Hf powder and Ta powder total mass, the quality of Si powder is 0.5% ~ 1% of Hf powder and Ta powder total mass, put into ball mill afterwards and be dry mixed more than 4h, add binding agent afterwards again and Hf-Ta alloy coat slip made by thinner, slip more than wet mixing 1h in ball mill;
Step (four), Hf-Ta alloy coat slip step (three) obtained are sprayed into the MoSi of product surface to be sprayed
2coatingsurface, puts into vacuum high temperature furnace by the product to be sprayed sprayed and sinters, and sintering temperature is 1850 DEG C ~ 1900 DEG C, insulation 10min ~ 20min, and during sintering, in stove, vacuum gauge pressure is less than 0.1Pa, heats up and terminates furnace cooling, make composite alloy coat.
In composite alloy coat preparation method on above-mentioned tantalum-tungsten alloy, the binding agent added in step () and step (three) is ethyl acetate, and thinner is zapon varnish.
In composite alloy coat preparation method on above-mentioned tantalum-tungsten alloy, at the MoSi of product surface spray coating to be sprayed in step (two)
2the thickness of coating paste is 150 μm ~ 250 μm, the MoSi after high temperature sintering
2coat-thickness is 80 μm ~ 120 μm.
In composite alloy coat preparation method on above-mentioned tantalum-tungsten alloy, at the MoSi of product surface to be sprayed in step (four)
2the thickness of the Hf-Ta alloy coat slip that coating sprays is 80 μm ~ 160 μm, and the thickness of the Hf-Ta alloy coat after high temperature sintering is 40 μm ~ 80 μm.
In composite alloy coat preparation method on above-mentioned tantalum-tungsten alloy, in step (two) and step (four), hydrocone type spray gun is adopted to carry out the spraying of slip.
In composite alloy coat preparation method on above-mentioned tantalum-tungsten alloy, the total thickness of the composite alloy coat that step (four) product surface to be sprayed is finally prepared is 120 μm ~ 200 μm.
In composite alloy coat preparation method on above-mentioned tantalum-tungsten alloy, MoSi
2powder, HfB
2powder, Hf powder, Ta powder, Y
2o
3the particle diameter of powder and Si powder is less than 50 μm, and purity is greater than 99.9%.
The present invention compared with prior art has following beneficial effect:
(1), the present invention adopts the MoSi prepared
2coating spraying at product surface as transition layer, at transition layer surface spraying Hf-Ta alloy coat, solve the oxidant protection under high temperature problem in conjunction with problem and tantalum-tungsten alloy of Hf-Ta alloy coat and body material, the coating uniform of preparation is fine and close, without the defect such as hole, crackle, and there is good antioxidant property;
(2), the present invention by lot of experiments to MoSi
2the proportioning of coating spraying slurry and spraying coating process, proportioning and the spraying coating process of Hf-Ta alloy coat slurry are optimized design, make the coating prepared have more excellent oxidation-resistance;
(3), test show, 1800 DEG C of static oxidation test life-spans of the composite alloy coat test piece that the present invention prepares, 1900 DEG C of static oxidation test life-spans, 1800 DEG C of dynamic air current washout test life-spans were more than 5 hours more than 10 hours more than 20 hours.
Accompanying drawing explanation
Fig. 1 is compound coating surface microscopic topographic prepared by the embodiment of the present invention 1.
Fig. 2 is compound coating surface microscopic topographic prepared by the embodiment of the present invention 2.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail:
Composite alloy coat preparation method on tantalum-tungsten alloy of the present invention specifically comprises the steps:
Step (one), MoSi
2coating Pulp preparation
Be the MoSi of 65% ~ 75% by mass percentage content
2powder and mass percentage content are the HfB of 25% ~ 35%
2powder mixes, and puts into ball mill and is dry mixed more than 4h, adds binding agent afterwards and MoSi made by thinner
2coating slip, slip more than wet mixing 1h in ball mill; Binding agent is ethyl acetate, and thinner is zapon varnish.
Step (two), MoSi
2coating high-temp sinters
By the MoSi that step () obtains
2coating slip adopts hydrocone type spray gun spraying to product surface to be sprayed, and thickness is 150 μm ~ 250 μm, and the coating of spraying wants even compact, without holiday.The product to be sprayed sprayed is put into vacuum high temperature furnace sinter, sintering temperature is 1850 DEG C ~ 1900 DEG C, insulation 10min ~ 20min, and during sintering, in vacuum high temperature furnace, vacuum gauge pressure is less than 0.1Pa, heats up and terminates furnace cooling, make MoSi
2coating, the MoSi prepared
2coat-thickness is 80 μm ~ 120 μm.
Step (three), Hf-Ta alloy coat Pulp preparation
By mass percentage content be 75% ~ 85% Hf powder and mass percentage content be 15% ~ 25% the mixing of Ta powder, then add Y
2o
3powder and the mixing of Si powder, wherein Y
2o
3the quality of powder is 0.5% ~ 1% of Hf powder and Ta powder total mass, the quality of Si powder is 0.5% ~ 1% of Hf powder and Ta powder total mass, put into ball mill afterwards and be dry mixed more than 4h, add binding agent afterwards again and Hf-Ta alloy coat slip made by thinner, slip more than wet mixing 1h in ball mill; Binding agent is ethyl acetate, and thinner is zapon varnish.
Step (four), Hf-Ta Alloy Composite Coating sinter
Hf-Ta alloy coat slip step (three) obtained adopts hydrocone type spray gun spraying to the MoSi of product surface to be sprayed
2coatingsurface, thickness is 80 μm ~ 160 μm, and the coating of spraying wants even compact, without holiday.The product to be sprayed sprayed is put into vacuum high temperature furnace sinter, sintering temperature is 1850 DEG C ~ 1900 DEG C, insulation 10min ~ 20min, during sintering, in stove, vacuum gauge pressure is less than 0.1Pa, heat up and terminate furnace cooling, make composite alloy coat, the Hf-Ta Alloy Composite Coating thickness prepared is 40 μm ~ 80 μm, and the total coat-thickness finally prepared is 120 μm ~ 200 μm.
MoSi in the present invention
2powder, HfB
2powder, Hf powder, Ta powder, Y
2o
3the particle diameter of powder and Si powder is less than 50 μm, and purity is greater than 99.9%, and vacuum high temperature furnace highest attainable vacuum gauge pressure is less than 10
-2pa.
Embodiment 1
To prepare Hf-Ta composite alloy coat on Ф 4.5 × 70mm coupon
(1) MoSi
2coating Pulp preparation
Select powder particle size to be less than 50 μm, purity is greater than 99.9%.
First by the MoSi of mass percentage content 65%
2powder, 35% HfB
2powder mixes, and puts into ball mill and is dry mixed 6h.Add ethyl acetate and suitable concn slip made by zapon varnish, wet mixing 1.5h in ball mill is for subsequent use for slip.
(2) MoSi
2coating high-temp sinters
Utilize hydrocone type spray gun that mixed slip is sprayed into specimen surface, thickness is 150 μm ~ 200 μm.The coating of spraying wants even compact, without holiday.
The sample sprayed is put into vacuum high temperature furnace sinter, sintering temperature 1850 DEG C, insulation 18min.During sintering, in stove, vacuum gauge pressure is less than 0.1Pa.Heat up and terminate furnace cooling, make MoSi
2coating, coat-thickness is 90 μm.
Vacuum high temperature furnace highest attainable vacuum gauge pressure is less than 10
-2pa.
(3) Hf-Ta alloy coat Pulp preparation
Select powder particle size to be less than 50 μm, purity is greater than 99.9%.
First by the Hf powder of mass percentage content 75%, 25% the mixing of Ta powder, then add the Y of 0.5%
2o
3powder and the mixing of 0.5%Si powder.Put into ball mill and be dry mixed 6h.Add ethyl acetate and suitable concn slip made by zapon varnish, wet mixing 1.5h in ball mill is for subsequent use for slip.
(4) Hf-Ta Alloy Composite Coating sintering
Utilize hydrocone type spray gun that mixed slip is sprayed into sample MoSi
2coatingsurface, thickness is 80 μm ~ 120 μm.The coating of spraying wants even compact, without holiday.
The sample sprayed is put into vacuum high temperature furnace sinter, sintering temperature 1850 DEG C, insulation 20min.During sintering, in stove, vacuum gauge pressure is less than 0.1Pa.Heat up and terminate furnace cooling, make Hf-Ta alloy coat, coat-thickness is 50 μm, and the composite alloy coat total thickness finally prepared is 140 μm.
Vacuum high temperature furnace highest attainable vacuum gauge pressure is less than 10
-2pa.
Be illustrated in figure 1 the compound coating surface microscopic topographic (500 times) prepared by embodiment 1 step (1) ~ step (4), the coating uniform prepared as seen from the figure is fine and close, without the defect such as hole, crackle.
1800 DEG C of 21 hours static oxidation test life-spans of composite alloy coat test piece, 1900 DEG C of 12 hours static oxidation test life-spans, 1800 DEG C of 6 hours dynamic air current washout test life-spans.
Embodiment 2
To prepare Hf-Ta composite alloy coat on Ф 4.5 × 70mm coupon
(1) MoSi
2coating Pulp preparation
Select powder particle size to be less than 50 μm, purity is greater than 99.9%.
First by the MoSi of mass percentage content 75%
2powder, 25% HfB
2powder mixes, and puts into ball mill and is dry mixed 6h.Add ethyl acetate and suitable concn slip made by zapon varnish, wet mixing 1.5h in ball mill is for subsequent use for slip.
(2) MoSi
2coating high-temp sinters
Utilize hydrocone type spray gun that mixed slip is sprayed into specimen surface, thickness is 200 μm ~ 250 μm.The coating of spraying wants even compact, without holiday.
The sample sprayed is put into vacuum high temperature furnace sinter, sintering temperature 1900 DEG C, insulation 18min.During sintering, in stove, vacuum gauge pressure is less than 0.1Pa.Heat up and terminate furnace cooling, make MoSi
2coating, coat-thickness is 110 μm.
Vacuum high temperature furnace highest attainable vacuum gauge pressure is less than 10
-2pa.
(3) Hf-Ta alloy coat Pulp preparation
Select powder particle size to be less than 50 μm, purity is greater than 99.9%.
First by the Hf powder of mass percentage content 85%, 15% the mixing of Ta powder, then add the Y of 0.5%
2o
3powder and the mixing of 0.5%Si powder.Put into ball mill and be dry mixed 6h.Add ethyl acetate and suitable concn slip made by zapon varnish, wet mixing 1.5h in ball mill is for subsequent use for slip.
(4) Hf-Ta Alloy Composite Coating sintering
Utilize hydrocone type spray gun that mixed slip is sprayed into sample MoSi
2coatingsurface, thickness is 120 μm ~ 160 μm.The coating of spraying wants even compact, without holiday.
The sample sprayed is put into vacuum high temperature furnace sinter, sintering temperature 1900 DEG C, insulation 20min.During sintering, in stove, vacuum gauge pressure is less than 0.1Pa.Heat up and terminate furnace cooling, make Hf-Ta alloy coat, coat-thickness is 70 μm, and the composite alloy coat total thickness finally prepared is 180 μm.
Vacuum high temperature furnace highest attainable vacuum gauge pressure is less than 10
-2pa.
Be illustrated in figure 2 the compound coating surface microscopic topographic (500 times) prepared by embodiment 2 step (1) ~ step (4).The coating uniform prepared as seen from the figure is fine and close, without the defect such as hole, crackle.
1800 DEG C of 25 hours static oxidation test life-spans of composite alloy coat test piece, 1900 DEG C of 13 hours static oxidation test life-spans, 1800 DEG C of 7 hours dynamic air current washout test life-spans.
The above; be only the embodiment of the best of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
The content be not described in detail in specification sheets of the present invention belongs to the known technology of professional and technical personnel in the field.
Claims (7)
1. the composite alloy coat preparation method on tantalum-tungsten alloy, is characterized in that: comprise the steps:
Step (one), be the MoSi of 65% ~ 75% by mass percentage content
2powder and mass percentage content are the HfB of 25% ~ 35%
2powder mixes, and puts into ball mill and is dry mixed more than 4h, adds binding agent afterwards and MoSi made by thinner
2coating slip, slip more than wet mixing 1h in ball mill;
Step (two), the MoSi that step () is obtained
2coating slip is sprayed into product surface to be sprayed, the product to be sprayed sprayed is put into vacuum high temperature furnace and sinters, and sintering temperature is 1850 DEG C ~ 1900 DEG C, insulation 10min ~ 20min, during sintering, in vacuum high temperature furnace, vacuum gauge pressure is less than 0.1Pa, heats up and terminates furnace cooling, make MoSi
2coating;
Step (three), by mass percentage content be 75% ~ 85% Hf powder and mass percentage content be 15% ~ 25% the mixing of Ta powder, then add Y
2o
3powder and the mixing of Si powder, wherein Y
2o
3the quality of powder is 0.5% ~ 1% of Hf powder and Ta powder total mass, the quality of Si powder is 0.5% ~ 1% of Hf powder and Ta powder total mass, put into ball mill afterwards and be dry mixed more than 4h, add binding agent afterwards again and Hf-Ta alloy coat slip made by thinner, slip more than wet mixing 1h in ball mill;
Step (four), Hf-Ta alloy coat slip step (three) obtained are sprayed into the MoSi of product surface to be sprayed
2coatingsurface, puts into vacuum high temperature furnace by the product to be sprayed sprayed and sinters, and sintering temperature is 1850 DEG C ~ 1900 DEG C, insulation 10min ~ 20min, and during sintering, in stove, vacuum gauge pressure is less than 0.1Pa, heats up and terminates furnace cooling, make composite alloy coat.
2. the composite alloy coat preparation method on a kind of tantalum-tungsten alloy according to claim 1, is characterized in that: the binding agent added in described step () and step (three) is ethyl acetate, and thinner is zapon varnish.
3. the composite alloy coat preparation method on a kind of tantalum-tungsten alloy according to claim 1, is characterized in that: at the MoSi of product surface spray coating to be sprayed in described step (two)
2the thickness of coating paste is 150 μm ~ 250 μm, the MoSi after high temperature sintering
2coat-thickness is 80 μm ~ 120 μm.
4. the composite alloy coat preparation method on a kind of tantalum-tungsten alloy according to claim 1, is characterized in that: at the MoSi of product surface to be sprayed in described step (four)
2the thickness of the Hf-Ta alloy coat slip that coating sprays is 80 μm ~ 160 μm, and the thickness of the Hf-Ta alloy coat after high temperature sintering is 40 μm ~ 80 μm.
5. the composite alloy coat preparation method on a kind of tantalum-tungsten alloy according to claim 1, is characterized in that: adopt hydrocone type spray gun to carry out the spraying of slip in described step (two) and step (four).
6. the composite alloy coat preparation method on a kind of tantalum-tungsten alloy according to claim 1, is characterized in that: the total thickness of the composite alloy coat that described step (four) product surface to be sprayed is finally prepared is 120 μm ~ 200 μm.
7. the composite alloy coat preparation method on a kind of tantalum-tungsten alloy according to claim 1, is characterized in that: described MoSi
2powder, HfB
2powder, Hf powder, Ta powder, Y
2o
3the particle diameter of powder and Si powder is less than 50 μm, and purity is greater than 99.9%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105386041A (en) * | 2015-12-10 | 2016-03-09 | 西北有色金属研究院 | Method for preparing modified composite Hf-Ta metal coating through laser cladding |
| CN105506427A (en) * | 2015-12-10 | 2016-04-20 | 西北有色金属研究院 | Tantalum alloy surface modified composite Hf-Ta coating layer and preparation method thereof |
| CN106242642A (en) * | 2016-07-28 | 2016-12-21 | 航天材料及工艺研究所 | A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof |
| CN106242643A (en) * | 2016-07-28 | 2016-12-21 | 航天材料及工艺研究所 | A kind of resistance to 1,300 1500 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof |
| CN105290389B (en) * | 2015-11-13 | 2018-02-06 | 航天材料及工艺研究所 | A kind of micro-satellite cluster thrust chamber slurry and its preparation method and application |
| CN112662978A (en) * | 2020-12-11 | 2021-04-16 | 郑州航空工业管理学院 | Coating for tungsten-copper alloy material and preparation method thereof |
| CN116219376A (en) * | 2022-12-23 | 2023-06-06 | 核工业理化工程研究院 | Tantalum surface high-temperature ablation resistant coating and preparation method thereof |
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| CN105290389B (en) * | 2015-11-13 | 2018-02-06 | 航天材料及工艺研究所 | A kind of micro-satellite cluster thrust chamber slurry and its preparation method and application |
| CN105386041A (en) * | 2015-12-10 | 2016-03-09 | 西北有色金属研究院 | Method for preparing modified composite Hf-Ta metal coating through laser cladding |
| CN105506427A (en) * | 2015-12-10 | 2016-04-20 | 西北有色金属研究院 | Tantalum alloy surface modified composite Hf-Ta coating layer and preparation method thereof |
| CN105386041B (en) * | 2015-12-10 | 2017-12-15 | 西北有色金属研究院 | A kind of method that laser melting coating prepares modified compound Hf Ta metal coatings |
| CN106242642A (en) * | 2016-07-28 | 2016-12-21 | 航天材料及工艺研究所 | A kind of resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof |
| CN106242643A (en) * | 2016-07-28 | 2016-12-21 | 航天材料及工艺研究所 | A kind of resistance to 1,300 1500 DEG C of low density carbon watt surface oxidation-resistant coatings and preparation method thereof |
| CN106242642B (en) * | 2016-07-28 | 2019-01-25 | 航天材料及工艺研究所 | Resistance to 1700 DEG C of low density carbon watt surface oxidation-resistant coatings of one kind and preparation method thereof |
| CN106242643B (en) * | 2016-07-28 | 2019-01-25 | 航天材料及工艺研究所 | A kind of resistance to 1300-1500 DEG C of low density carbon watt surface oxidation-resistant coating and preparation method thereof |
| CN112662978A (en) * | 2020-12-11 | 2021-04-16 | 郑州航空工业管理学院 | Coating for tungsten-copper alloy material and preparation method thereof |
| CN112662978B (en) * | 2020-12-11 | 2023-03-24 | 上海理工大学 | Coating for tungsten-copper alloy material and preparation method thereof |
| CN116219376A (en) * | 2022-12-23 | 2023-06-06 | 核工业理化工程研究院 | Tantalum surface high-temperature ablation resistant coating and preparation method thereof |
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